CN102786566B - Method for absorbing and purifying stevioside through multiple-column secondary resin series connection - Google Patents

Abstract

The invention discloses a method for absorbing and purifying stevioside through multiple-column secondary resin series connection. Smashed stevia rebaudiana leaves are subjected to processes such as preprocessing, desalinization, primary absorption and analysis, decoloration, primary ion exchange, secondary absorption and purification, secondary ion exchange, spraying and drying, and a high-purity stevioside product is obtained. The impurities in the stevioside are absorbed through TH-3 absorption resin, the stevioside content of effluent liquid is improved, the stevioside is purified, the glycosides content of the stevioside product can achieve more than 95% and the absorbency is no more than 0.03.

Description

The method of multicolumn secondary resin series connection absorption purification Steviosides

Technical field

The present invention relates to a kind of preparation and purification techniques of Steviosides, especially a kind of method of multicolumn secondary resin series connection absorption purification Steviosides.

Background technology

Stevioside product is from catananche--a kind of high sugariness extracted the blade of sweet Stevia, low calorie, taste matter are good, the extraordinary a kind of novel pure natural sweeting agent of safety non-toxic, market outlook; The industries such as food, beverage, medicine, daily chemical industry can be widely used in.Steviosides is polycomponent glucoside mixture, and sweet ingredient known at present has 9 kinds, and its sugariness and mouthfeel depend on glucoside component and total glycoside content.At present, the market requirement containing the high purity stevioside product of glucoside amount >=95% is increasing, by world market is pursued, but its purity of product that the production purifying technique of existing stevioside product is produced is namely containing glucoside amount≤90%, is difficult to reach world market requirement.

Summary of the invention

The object of the present invention is to provide a kind of multicolumn secondary resin to connect and adsorb the method for purification Steviosides.

The technical solution adopted for the present invention to solve the technical problems is:

(a) pre-treatment: the stevioside leaf pulverized is mixed with 50 DEG C of-55 DEG C of softening waters, continuous countercurrent extraction, makes the glucoside percentage extraction of stevioside leaf reach more than 99.99%, makes Steviosides extraction liquid, extraction liquid, after flocculation sediment and filter press two procedures, enters next process;

(b) desalination: by the desalination of above-mentioned filtrate spent ion exchange resin, obtain the desalination filtrate of transmittance >=65%, specific conductivity≤6700us/cm, desalination filtrate enters next process;

(c) primary sorption and parsing: adopt Steviosides effective constituent in the above-mentioned desalination filtrate of resin absorption, when going out sweet to resin only; With dilute solution of sodium hydroxide, hydrochloric acid dilute solution, pure washed resin, to reach 7 to effluent liquid pH value time only; By concentration be 52% ethanolic soln point post carried out to resin resolve, must be that desorbed solution enters next process containing glucoside amount at 82-86%, desorbed solution than absorbancy≤0.50 containing glucoside amount;

D () is decoloured: gac is inserted mix and blend in desorbed solution, Plate Filtration filter containing glucoside amount at 83-87%, destainer than absorbancy≤0.20, destainer enters next process;

(e) primary ions exchange: destainer successively by after Zeo-karb and anionite-exchange resin removal of impurities, evaporation concentration, obtain containing glucoside amount at the concentrated solution of 84-88% than absorbancy≤0.10, concentrated solution enters next process;

F () second adsorption removal of impurities: adsorb above-mentioned concentrated solution removal of impurities with the supersaturation of LX-18 polymeric adsorbent three columns in series, flows out Steviosides solution, obtain containing glucoside amount >=95%, Steviosides effluent liquid than absorbancy≤0.03, effluent liquid enters next process;

(g) Two-step ion-exchanging: the Zeo-karb and the anionite-exchange resin that effluent liquid are entered again dormant state carry out deep impurity-removing, nanofiltration membrane concentrates and obtains containing glucoside amount >=95%, concentrated solution than absorbancy≤0.03, again through degerming filter membrane Sterile Filtration, concentrated solution enters next process;

H () spraying dry: by the concentrated solution spraying dry after Sterile Filtration, obtains containing glucoside amount >=95%, stevioside product than absorbancy≤0.03.

Effect of the present invention is: utilize TH-3 polymeric adsorbent adsorb the impurity in Steviosides thus improve the Steviosides content in effluent liquid, reach the object of purification Steviosides, last gained stevioside product reaches more than 95%, than absorbancy≤0.03 containing glucoside amount.

Embodiment

Below in conjunction with embodiment, the present invention is described in further detail.

(a) pre-treatment: mixed by weight 1:15 with 50 DEG C of-55 DEG C of soft water by Stevia leaves, make Steviosides extracting solution, through flocculation sediment and filter press two procedures, the filtrate after Plate Filtration enters next process;

(b) desalination: by the desalination of above-mentioned filtrate spent ion exchange resin, obtain the desalination filtrate that transmittance is 78.3%, specific conductivity is 5875us/cm, desalination filtrate enters next process;

(c) primary sorption and parsing: adsorb Steviosides effective constituent in above-mentioned desalination filtrate with HT-3 type polymeric adsorbent, the absorption treated rear discharge up to standard of waste liquid or reuse, after having adsorbed the resin of Steviosides effective constituent with the sodium hydroxide solution of 0.5% of 2BV resin volume and 0.5% hydrochloric acid soln process of 2BV resin volume, employ alkali at every turn, acid all needs the pure water drip washing resin with 2BV resin volume, stop when effluent liquid pH value reaches 7, resolve with 52% ethanolic soln of 2BV resin volume again, obtain containing glucoside amount 84.5%, be the desorbed solution of 0.434 than absorbancy, desorbed solution enters next process,

D () is decoloured: will to insert in desorbed solution mix and blend 1 hour by desorbed solution volume ratio 0.04% vegetable active charcoal, and filter be 84.8% containing glucoside amount, be the destainer of 0.179 than absorbancy, destainer enters next process;

(e) ion-exchange: destainer is successively by 732 type Zeo-karbs and the removal of impurities of LK-330 anionite-exchange resin, and it be 85.3% is the once concentration liquid of 0.086 than absorbancy that evaporation concentration obtains containing glucoside amount, and concentrated solution enters next process;

(f) second adsorption: adsorb above-mentioned ion exchange liquid with the extraordinary polymeric adsorbent three columns in series of LX-18, obtain the effluent liquid after supersaturation, effluent liquid enters next process;

(g) Two-step ion-exchanging: effluent liquid is entered again processed 732 good type Zeo-karbs and YW-07t type anionite-exchange resin carries out deep impurity-removing, concentrate through nanofiltration and obtain being 95.8% containing glucoside amount, being the Two-step ion-exchanging liquid of 0.013 than absorbancy, carry out degerming filter core Sterile Filtration again, sterile liquid enters next process;

(h) spraying dry: sterile liquid is carried out spraying dry, obtains stevioside product.Through efficient liquid phase chromatographic analysis, product is 95.88% containing glucoside amount, is 0.013 than absorbancy.

The present invention and traditional technology and industry mean level (ML) are compared as follows:

Technical indicator (what do not indicate especially is mean value)	Traditional technology	Technique after improving	Industry mean level (ML)
				Than absorbancy ( ）	0.08	0.04	0.08
Containing glucoside amount (%)	90	≥95	90
				Impurity ratio (%)	7.8	1.5	7.8

In literary composition, the measuring method of each parameter is:

(1) containing the detection method of glucoside amount and purity: by JECFA 2010 Steviol Glycosides;

(2) determination of light transmittance method: room temperature 25 DEG C of 722 type visible spectrophotometer wavelength 480 nanometer;

(3) conductance measurement method: room temperature 25 DEG C of conductivitimeters;

(4) than absorbance measurement method: by GB 8270-1999.

Claims (1)

1. a method for multicolumn secondary resin series connection absorption purification Steviosides, its feature is as follows in preparation method:

(a) pre-treatment: the stevioside leaf pulverized is mixed with 50 DEG C of-55 DEG C of softening waters, continuous countercurrent extraction, makes the glucoside percentage extraction of stevioside leaf reach more than 99.99%, makes Steviosides extraction liquid, extraction liquid, after flocculation sediment and filter press two procedures, enters next process;

(b) desalination: by the desalination of above-mentioned filtrate spent ion exchange resin, obtain the desalination filtrate of transmittance >=65%, specific conductivity≤6700us/cm, desalination filtrate enters next process;

(c) primary sorption and parsing: adopt Steviosides effective constituent in the above-mentioned desalination filtrate of resin absorption, when going out sweet to resin only; With dilute solution of sodium hydroxide, hydrochloric acid dilute solution, pure washed resin, to reach 7 to effluent liquid pH value time only; By concentration be 52% ethanolic soln point post carried out to resin resolve, must be that desorbed solution enters next process containing glucoside amount at 82-86%, desorbed solution than absorbancy≤0.50 containing glucoside amount;

D () is decoloured: gac is inserted mix and blend in desorbed solution, Plate Filtration, filter containing glucoside amount at 83-87%, destainer than absorbancy≤0.20, destainer enters next process;

E () primary ions exchanges: destainer successively by after Zeo-karb and anionite-exchange resin removal of impurities, evaporation concentration, obtain containing glucoside amount at 84-88%, concentrated solution than absorbancy≤0.10, concentrated solution enters next process;

F () second adsorption removal of impurities: adsorb above-mentioned concentrated solution removal of impurities with the supersaturation of LX-18 polymeric adsorbent three columns in series, flows out Steviosides solution, obtain containing glucoside amount >=95%, Steviosides effluent liquid than absorbancy≤0.03, effluent liquid enters next process;

(g) Two-step ion-exchanging: the Zeo-karb and the anionite-exchange resin that effluent liquid are entered again dormant state carry out deep impurity-removing, nanofiltration membrane concentrates and obtains containing glucoside amount >=95%, concentrated solution than absorbancy≤0.03, again through degerming filter membrane Sterile Filtration, concentrated solution enters next process;

H () spraying dry: by the concentrated solution spraying dry after Sterile Filtration, obtains containing glucoside amount >=95%, stevioside product than absorbancy≤0.03.